HRID1684035

反应详情

EQUATION

反应方程式

HRID 1684035 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Trans-2-(3,4-dimethoxy-5-nitrophenyl)-4-(3,4,5-trimethoxyphenyl)-1,3-dithiolane (2) (FIG. 20) (3.10 g, 6.84 mmole) was predissolved in 33 ml absolute ethanol. To this solution was added calcium chloride (0.721 g, 6.50 mmole) predissolved in 7 ml H2O followed by freshly activated zinc dust (10.0 g,195 mmole). The reaction was refluxed for 12 hours. The solid was removed by vacuum filtration through celite and was washed with ethyl acetate. The filtrate was washed with H2O, dried over MgSO4, and evaporated in vacuo to a white foam (2.52 g, 87%).

WORKUP

后处理

  1. temperatureThe reaction was refluxed for 12 hours
  2. customThe solid was removed by vacuum filtration through celite
  3. washwas washed with ethyl acetate
  4. washThe filtrate was washed with H2O
  5. dry with materialdried over MgSO4
  6. customevaporated in vacuo to a white foam (2.52 g, 87%)